Suspensions and method for their production



Jan. 10, 1939. s. .1. WYNN 2,143,099

SUSPENSIONS AND METHOD FOR THEIR PRODUCTION Filed June 19, 1954 4 Sheets-Sheet l ATTORNEYS Jan 10, 1939. s. J. WYNN I 2,143,099

SUSPENSIONS AND METHOD FOR TEEIR PRODUCTION Filed June 19, 1934 4 Shets-Sheet 2 L v I ENTOR ATTORNEYS Jan. 10, 1939. s. J. WYNN w2,143,099

SUSPENSIQNS AND METHOD FOR THEIR PRODUCTION Filed June 19, 1954 4 sneets sheet 5 14 v 8 IAPVAE/NTOR ATTORNEYS Jan. '10, 1939. 5. J. WYNN 2,143,099

SUSPENSIONS AND METHOD FOR THEIR PRODUCTION 1 Filed June 19, 1954v 4 Sheets-Sheet 4 wady agizza" y Wm ATTORNEYS Patented Jan. 10, 1939 PATENT orrics susrENsmNs AND METHOD non 'rnnm. rnonucrron Samuel Joseph Wynn, New York, N. Y., assignor to Colloid Corporation, Baltimore, Md a corporation of Maryland Application June 19, 1

. 5 Claims.

The present invention relates to novel suspensions and to a novel method for producing the same, it being understood that the term suspension as used herein should be taken to mean a composition of matter comprising subdivided particles ormicells of one or more substances in one or more other substances, which subdivided particles or micells are larger than molecular in size and either colloidal or larger than colloidal in size.

Certain types of suspensions and particularly emulsions, as made by existing methods, have lacked one most desirable property. They cannot be diluted to any useful extent. That is, material of the outer phase or of the character of the outer phase cannot be added to produce dilution in the proportions often desired. This limitation is necessitated by the very nature of these suspensions. The protective colloid or peptizing agent required by current methods is generally soluble in the material required for dilution or may be peptized by such material with the result that, if dilution is carried beyond a certain limit, a breakdown or separation of phases takes place. Obviously, other means of securing stability must be sought if it is desired to adjust the ratio of inner to outer phases of such suspensions'sub-- sequently to their preparation. One such means would be to so reduce particle size of the inner phase that Brownian motion and the forces of surface energy may supplant entirely or in part the function of protective colloids or peptizing agents in achieving to a practical degree both stability and dilution.

In accordance with the invention use is made of a method of impactive treatment resulting in an extremely fine subdivision of the matter to be dispersed in the-outer phase. Suspensions may thus be produced characterized by their freedom or substantial freedom from protective colloids or agents effecting or promoting dispersion, depending for stability upon extreme minuteness of the suspended particles. These suspensions are capable of dilution or naturally difiusible in the material constituting the outer phase or material of the character of the material constituting the outer phase. Moreover, when of the oil-in-water type, they may be concentrated by distillation under reduced pressure. Still another advantage resides in the fact that, when the suspended particles are not all of colloidal character, protective colloids or dispersion promoting agents may be employed subsequent to actual production by the impactive treatment.

The invention will be understood with the aid 934, Serial No. 731,390

of the following description taken in connectio with the accompanying drawings in which Fig. is a schematic illustration of a device for demo! strating the effects of my novel method of treal ment; Fig. 2 is a profile view of an apparat1 for carrying out the treatment in practice; Fig. is a longitudinal cross-sectional view taken 0 the plane indicated by the line 3 4) in. Fig, 2 Fig. 4 is an enlarged detail view, in cross-sectioi of the lower end of the plunger; Figs. 5 and are plan views of two different forms of vibratin elements; Fig. 7 is a view, on a reduced scale, an agitating device for effecting preliminary mi: ing; Figs. 8 and 9 are, respectively, profile an front views of another apparatus constructed f( commercial use of the invention; Fig. 10 is a vie of still another apparatus constructed for con merical use of the invention; Fig. 11 is an er larged detail view of the container-actuating gez employed in the apparatus shown in Fig. 10; Fig 12 and 13 are illustrative of standing tests pei formed with oil-in-water mixtures; and Figs. 1 l5 and 16 are illustrative of standing tests pei formed with magnesium hydroxidesuspension I have made the important discovery that whe two contacting substances are subjected to in pactive energy externally efiected between. tw repeatedly impacting rigid bodies and mechan: cally delivered through vibrating elements to tr substances, one will be thrown into an extreme] fine state of dispersion into the other, provided, course, the substances are of such nature as i permit their admixture in this manner. Th: phenomenon may be readily observed with the ai of the device shown in Fig. 1. Referring to th figure, the numeral l indicates a plate of vibratil material which carries an adjustable armature at one end and is'secured by a flexible member to a basefi. An iron-core electromagnet 6 is or eratively associated with the armature 2 in suc a manner that successive impacts between arms ture and core will take place when alternatin current is passed through its coil. To assist re traction, an adjustable-tension spring 1 may t employed as shown. A film of oil 9 is even] spread over the upper surface of the plate I am while the impacts are being delivered, a sma quantity of pure distilled water l0 deposited upo the oil film soon becomes cloudy in appearanc showing that'a dispersion of some of the oil ini the water has taken place. Suspensions create in this manner, after mechanical separation suc as vacuum filtration through tight paper, exhib true colloidal properties. For example, a Tynda light cone can be formed therein by using proper lens and light source. Also, a microscopic inspection with direct illumination will show an absolutely clear field up to 900 diameters, but with a dark field condenser at open diaphragm position will show a few particles with the field exhibiting luminescence. In the ultramicroscope a profuse dispersion of particles in active Brownian movement is found with the particle sizes ranging from 0.2; downward to limits of visibility in such device. Such suspensions can be diluted to any desired extent. Dilution of a given specimen into optically clear distilled water to the extent of 2 parts of specimen to 1,000,000 parts of water will still produce a definite light cone, whereas none is in evidence in the water prior to admixture of the specimen therewith.

It now becomesapparent that the disruptive efi'ect produced in matter by the impactive treatment above stated may be employed to create entirely new suspensions of a colloidal character. By this novel treatment matter in either liquid form or in solid particle form may be dispersed into a liquid phase with great effectiveness and without the assistance of either protective colloids or peptizing substances. In fact, the presence of certain colloids, certain gums for example, inhibits the dispersion or lessens the effectiveness of the treatment.

In each of the apparatus which will be presently described, the impactive energy required for the treatment is derived from the successive impacts of an armature upon an iron-core electromagnet energized'by alternating current and is communicated to the substances to undergo treatment through a system of spaced vibrating elements immersed therein. I

Referring to Figs. 2 and 3, an elongated container II is provided for containing the bodies to undergo treatment, it being held in-a vertical position by an upright panel l2 having a base l4. It may be conveniently formed by a pipe l5 and-bottom cap l6 screw-threaded to one another, both pipe andcap being of massive construction. A drain-cock H of standard construction is screw-threaded into a central opening l9 formed through the bottom piece I6 and serves to draw ofi the treated contents. Any suitable means may be used for attaching the container H to the panel l2 and in the apparatus illustrated bolts 20 are screw-threaded into bosses 2| formed on the pipe l5, collars 22 providing the proper spacing between container and panel. The bodies may, if desired, be directly poured into the container II at its top, but they should preferably be introduced in a state of preliminary admixture, which may be eflected in any well known manner. Thus in Fig. 7 a container 24 is shown, wherein the bodies may be caused to undergo preliminary agitation by a motor-driven propeller 25, a funnel 26 being provided for introducing the bodies therein. A pipe or conduit 21 leads from the container 24 to the top of the container II, a valve 29 being able rod or vertical plunger 34, the lower end portion 35 of which is enlarged and loosely engages 'the opening IS, the whole series of discs and spacers being rigidly supported between two clamping collars 36 and 31. As will be seen, the plunger 34 at its lower extremity normally abuts the upper end of the drain-cock l1, and, as best shown in Fig. 4, its lower portion 35 is formed with radial inlets 39 and a central opening 40 communicating therewith to provide an exit passage for the treated bodies when withdrawing them from the container through the draincock l1. Suitable perforations are formed through the discs 3| to facilitate fluidcirculation in the container two possible forms of opening, namely, round and square, being shown in Figs. 5 and 6, respectively. A compression spring 4| is fitted over the plunger portion 35 between cap l6 and collar 36. I

The electromagnet 42 which serves with the armature 43 to impart energy through the system 30, is conveniently mounted on a platform 44 in the rear of the panel 62, it being provided with terminals 45 for connection to a suitable source-of alternating current (not shown). The armature 43 is juxtaposed to the electromagnet core 45 on an arm 41 pivotally connected to a bracket 48 secured to the panel |2. The arm 41 extends through an opening 49 in the panel and is pivotally connected to another bracket.

50 to which the upper end of the plunger 34 is rigidly secured, it being noted that the pivotal connection between the arm 41 and the bracket 50 is such as to preclude or substantially preclude any lost motion. A tension spring 5| is connected between the outer end of the arm 41 and a tension-adjusting screw 52 carried bya bracket 54 secured to the panel l2, a nut 55 being provided on the screw to lock it in any position of adjustment. a

It is apparent that any impactive force applied to the armature 43 will be transmitted to the system 30 in the container That is, these parts are conjointly movable because of their mutual connection with the pivotal arm 41.

It is also apparent that the respective actions of the two springs 4| and 5| are opposite to oneanother. That is, the compression spring 4| tends to produce upward movement of the system 30 and downward movement of the. arms;- ture 43 and the tension spring 5| tends to produce downward movement of the system 30 and upward movement of the armature 43. Now the spring 5| is of greater strength than the spring 4| so that, with no current flowing in the electromagnet 42, the plunger 34 is caused to contact at its lower end portion 35 with the drain-cock l1 acting as a stop, and, for this position of the plunger, the armature 43 is spaced from the core 46. Upon energization of the electromagnet, the armature 43 is pulled downward against the force of the spring 5| and the tension of the latter 1 is then adjusted, by means of the set screw 52,

to cause periodic impacts of desired intensity to take place between the members 43 and 46. During operation, the plunger 34 does not come in contact with the drain-cock I! because of the inertia of the treated bodies andtheir damping eflect on theelements 3|. I

It has been found that in some cases heating the bodies while they undergo treatment assists the dispersion contemplated. Thus, a coil 55,-

ner as by bolting it to the panel l2 as illustrated, collars 59 providing a spacing between coil and panel. It is understood, of course, that the coil 56 is designed to provide moderate heat only. That is, the temperature in the container-ll should not be raised to the point where vaporization of either of the components or phases undergoing treatment will be caused.

The apparatus shown in Figs. 8 and 9 is essentially the same as that'of Figs. 2 and 3, but in addition comprises means for simultaneously oscillating and rotating the container Thus the bottom piece It is formed on its bottom surface with. peripheral teeth 60 meshing with an elliptical gear 8|, which is rotated through a suitable speed-reducing gearing mechanism 62 by a motor 84 fixed to the base It, the container b eing guided for oscillatory and rotary movement by annular elements or collars 65 having lateral I the plunger, block 88 contacts at any instant with extensions 86 by means of which they may be bolted to the panel" I2. In this manner increased agitation of the bodies in the container II is obtained, which permits the treatment to take effeet on a more even distribution of inner phase, as well as on an increased amount of innerphase in suspension. Further, the renewing of the surface of contact between the bodies and the elements 3| is more rapid and more effectively executed as well.

By means of the apparatus shown in Fig. 10, the treatment may be carried out under pressure, this also having been found, in some instances, to assist the dispersion. A flexible diaphragm I is interposed between the pipe l5 and a cap 1| screw-threaded to the pipe a]; its upper end, a packing 12 being provided to prevent pressure release during operation. The plunger 34 extends through the diaphragm 10, but has an air-tight connection therewith. The bodies to undergo treatment are introduced through a nipple 74 screw-threaded into the wall I5, which nipple M is provided with a valve 15 which is closed after introduction of said bodies. Suitable air pressure is then applied through a nipple 16 also screw-threaded into the wall l5, which nipple I6 is also provided with a valve 11, subsequent closure of which prevents release of the applied pressure. To off-set the effect of pressure on the diaphragm 10, a. spring 19 is interposed between said diaphragm and an upper cap 80 screw-threaded'to the cap 1|. As in Figs. 8 and 9, means are provided for rotating and oscillating the container II, it being understood that the bodies to undergo treatment and the-air-pressure are supplied to the nipples l4 and I6 through flexible conduits (nrt shown), which are detached from said nipples prior to imparting motion to the container. Here the peripheral teeth 88 formed on the bottom piece l6 mesh with a gear 8| which is so constructed that the oscillatory movement of the container is caused to take place intermittently. Referring to Fig. 11, the major portion 82 of the gear 8| follows a circular pitch-line, while the remaining portion 84 follows'a pitch-line within the circle 85 drawn through the pitch-line of the portion 82, it being particularly noted that by this construction the container is held in an uppermost. position for a predetermined period of time, whereupon it is lowered and raised back to its uppermost position. The plunger 34 here moves with the container I, which necessitates a modified construction for .transferring through said plunger the impactive energy required for treatment of thebodies in the container. Thus, the plunger 34 is secured at its upper end to a block 88 having a rounded surface adapted to rotatably engage a depression 81 in the pivotal arm 89 when the apparatus is in operation and the container II is in its uppermost position, the armature 98 carried by the pivotal arm being here attracted upwardly by the electromagnet 9| against the force of the tension-adjustable spring 92. A stop 94 determines the normal position of the arm 89. Before energizing the electromagnet 9|, the container israised, if necessary, to its uppermost position and in this position its rotation is stopped.

Alternating current is then passed through the electromagnet 9| and by proper adjustment of the screw determining the tension of the spring 92 successive impacts are caused to take place between the armature 90 and the electromagnet core 95. As long as the container II is caused to remain stationary in its uppermost position,

the arm 89, so that impactive energy is continuously communicatedthrough the plunger and discs 3| mounted thereon to the bodies in the container. With the motor 84 running, however, the motion of the container causes the plunger block 86 to move in and out of contact with the arm 89, so that impactive treatment is effected intermittently. The container II is rotated continuously, impactive treatment being effected during the periods that the plunger block 86 rotatabl'y engages the arm 89 and oscillatory movement of the container being effected during the shorter interval that the plunger block 88 is out of contact with the arm 88. It should be observed that, in view of the resilience of the diaphragm 18, there is relative movement between the elements 3| and the container each time the block 88'moves either in or out of contact with the arm 89, because of which renewal of the surface of contact between bodies and elements 3| is similar to that executed in Figs. 8 and 9. Observing that the boiling points of liquids increase with increasing pressure applied thereon, the apparatus of Fig. 10 provides the further advantagethat higher temperatures may be employed.

The period of time required for. effecting dispersion in either of the apparatus embodiments which have been described depends on such factors as the nature of the bodies treated, the amount of inner phase to be dispersed and the contemplated stability of the dispersion. Thus, a period of, say,

5 to minutes may be found suflicient for some treated in a continuous flow through the container That is, the bodies may be continuously fed to the container H and continuously discharged therefrom.

Examples will now be given of some commercial products which may be made in accordance with the invention.

Example 1 able the impactive treatment to be effective. The

material is then permitted to run into the con tain'er II of, say, Figs. 2 and 3, wherein it is treated for a period'of 1 to 20 minutes. II desired, the material may be slightly heated during this treatment. The material is then withdrawn from the-container II and again agitated for about minutesin the container 24 with another 1% of the same oil, whereupon the resulting material is subjected to'impactive treatment in the container II for anotherperiod of to minutes,

heat being again employed if desired. This procedure is repeated, each 7 time adding a, small quantity of the same oil, until approximately 5%. y of oil has been added to the water phase andtreated therewith. The material may then be introduced through the drain-cock I1 into the separatory funnel I00 shown in Fig. 12 and, after a standing period of i to2 days therein, it will be found to have thenovel appearance illustrated.

Zone IN is an upper layer of free oil which may represent from '10 to 20% of the total amount of oil used, zone I02 is a creamy layer of fine particles of oil suspended in water, and zone I03 is a permanent I .colloidal solution of oil in water. There is no clear water zone. An analysis of the material of any zone will show no chemical change has taken place (for certain oils oxidation may take place, but with'mineral oil this is negligible). A quantitive determination of the materialof zone i0; will show about, two percent of oil in suspension. The material of zone I02 consists mainly of particles somewhatlarger than in the colloidal material ofzone I03, but both the material of zone I02 and the material of zone I03 are capable of dilution in aqueous media. material of zone, I02, if collected, also constitutes a valuable product since it assays 60 to 70% oil.

Its stability can be increased by the addition of a protective colloid or by the addition of almost any substance which will reduce the surface tension of the water phase. Any substance which will increase the hydroxyl-ion concentration will likewise restrain aggregation. As an example of stabilization by the protective colloid method, addition of a solution of gum acacia to cause the material of zone I02 to contain 0.02% of said gum will'stabilize said material for a period of six months or more. As an example of stabilization by reduction of surface tension, addition of 5 parts of a 5% soap solution .to 95 parts of said material will provide stability for at least the same period. As an example of stabilization by increase of the hydroxyl-ion concentration, addition of ammonium hydroxide to produce a pH of 7.15

will again provide stability for at least the same period. In its stabilized state, the material of zone I02 is still capable of dilution in aqueous media, this being due to the very small quantity of protective colloid or other agent-necessary to increase its stability, but'also due to the fact that its oil particles are close to colloidal size (its period of stability without stabilizingagents therein is two weeks or more). The free oil in zone IOI represents the agglomeration of particles which have not be n suificiently comminuted by the impactive treatment. It should be observed that there is a certain amount of oil which clings to certain parts of the apparatus from which no impactive energy The is transmitted,thus constituting freeor untreated material.

The novel character of the suspensions created in accordance with this invention may be readily appreciated by comparison with the totally different results obtained by standing of mixtures produced by ordinary means in the absence of protective colloids. The following test has been made with this comparison in View.

Comparative test The identical procedure given in Example 1 is repeated, except that-here a-colloid mill of the type employing both high shearing stress and high beating action is employed instead of the apparatus of the present invention. That is, purified white mineral oil and distilled water are alternately agitated and treated in suchmill for the same periods of time, the amount of .011 being as before gradually increased until an approximate oil concentration of 5% is reached. For a true comparison with the material obtainedin Exampie 1, no protective colloid or third substance should be employed and as before all apparatus,

should be: chemically clean. Fig ,13 I illustrates the appearance of the final mixture obtained in this manner after a standing period of 1 to 2 days in the separatory-funnel I04. Zone I05 is as before free oil, but here represents perhaps 99% of the total amount employed; zone I06 is cloudy with minute water drops suspended in oil; zone I01: is also cloudy, but with minute oil drops suspended in water; and zone I08 is clear water. Neither the material of zone I06 nor the material of zone I01. isof a colloidal character. That is, theoil droplets in zone I01. agglomerate and rise through the zone I05 into the free oil zone I05,

whereas the water droplets in zone I06 agglonien ate and sink through the zone I01 into the free I water zone I08. After a further standing period of a day or so, both zone I06 and zone I 01 will dis-'- appear. That is, the oil and water phases will then be in the same condition as they were priorto admixture.

Since most protective colloids are affected by heat, either physically or chemically, it is apparent that it has not heretofore been possible to employ distillation for increasing the concentration of emulsions. On the other hand, the novel oil-inwater suspension obtained by my impactive treatment may be further concentrated by distillation under reduced pressure. For example, vacuum distillation of the colloidal solution of mineral oil in water obtained in Example 1 (zone I03) has in actual practice yielded concentrates of 3.6% oil content. It should be observed that .this figure was attained with a pH of 7.0 and with Example 2 Three parts of cod liver oil, which may have been treated to have a. high vitamin content, and 100 parts of distilled water are agitated in the container 24 for about 5 minutes, whereupon the mixture is subjected to impactive treatment in the container II of, say, Figs. 8 and 9, for about 15 minutes. The treated mixture-is then drawn oil? and again agitated for about 5 minutes in the container 34 with 3 more parts of the same oil, whereupon the resulting mixture is subjected to impactive treatment in the container H for a further period of about 15 minutes. This procedure is repeated, each time adding 3 more parts of the same oil, until 18 parts in all have been added to the water phase and treated therewith. The material withdrawn after the last treatment in the container II is allowed to stand for about 2 days during which the three zones shown in Fig. 12 will have formed. The suspensions corresponding to the zones Hi2 and H13 are then separately collected. The creamy layer corresponding to zone W2 contains about 66% oil and does not show any sign of breaking down for a period of at least two weeks. It may, of course, be permanently stabilized by addition of a protective colloid and, in this state, it is still capable of dilution in water. The suspension corresponding to zone M33 contains about 2% of oil in permanent dispersion.

Attempts have been made to introduce cod liver oil concentrates into mill; by the hcmogenizer. Millrcontains casein and albumen as protective colloids, but in actual practice the mixtures cbtained in this manner have not been homogeneous to the extent that is desired. Now either one of the cod liver oil suspensions obtained in Examplefri, i. e., either the colloidal solution corresponding to zone M3 or the suspension corresponding to zone N32, may be simply added to the milk or, in fact, to any aqueous foodstuff, with satisfactory homogeneity of the final products.

3 have also discovered that, in the preparation of oil-in-water suspensions in the fcrm'or zone '15?- of Fig. 12, their stability may be considerably increased if there is added to the oil, prior to its dispersion, a substance which is soluble therein and of a higher specific gravity. Substances such as lecithin have been found admirably suited for this purpose. These substances, in addition to weighting down the oil, also iunc tion as anti-ox dants.

Example 3 One part or lecithin is added to 99 parts of end liver oil, which may have been treated to have a high vitamin content. The resulting mixture may then be treated with distilled water in ac cordance with the procedure given in Example 2. The creamy layer (zone M2) obtained in this manner shows no sign of breaking down whatever and a chemical analysis after weeks of stand ing and exposure to light will show no oxidation of the oil. Its subsequent addition to milk constitutes a very valuable product.

Example 4 An essential oil is dispersed in distilled water by the practice of this invention and the colloidal solution thus obtained (zone W3) is then vacuum distilled. The distillate, while apparently clear to the eye, contains in colloidal solution an amount of oil which renders it suitable for the preparation of toilet water, hand lotions, hair tonics and the like. The main advantage here is the avoidance of the use of alcohol which is considered deleterious in its effect upon the skin and scalp. Economy in cost of preparation is another advantage. The residue from distillation is also a valuable product containing in permanent suspension a higher percentage of the essential oil than the transparent solution obtained as a distillate. This residue may be used without further treatment. Both the distillate and the residue, as well as products derived therefrom, are soluble in water.

Example 5 Water, as the inner phase, is temporarily suspended in gasoline by agitation and. the temporary mixture thus formed is subjected to impactive treatment in accordance with this invention. The treated material is then drawn off and centrifuged or permitted to stand until all excess water has settled out. The colloidal solution thus obtained is an excellent fuel for internal combustion engines. Increases in efiective power delivery up to 40% have been recorded.

Example 6 The invention may be used for decolorizing matter. Thus, an organic material of an oily nature and containing an undesirable coloring substance is suspended in water in accordance with this invention. Should the material be too viscous at normal temperature, the treatment may be carried out at the temperatures provided by the heating coil as and if necessary under pressure by the apparatus of Fig. 10. If the material is still too viscous to suspend, it may be first dissolved in a predetermined amount of neutral solvent. By breaking me suspension thus formed, a great deal of the coloring substance will be precipitated in the aqueous phase and the recovered material, which rises to the top, will be free or substantially free therefrom.

That is, the material may be freed, by the procedure given, of decolorizing matter to the extent required for its proper use.

Example 7 $01118 dyestufis which are insoluble in water, are soluble in oil, but can be made water soluble in accordance with the invention. The oil soluble dye is dissolved or peptized in a suitable oil and the resulting material is in turn suspended in water in accordance with the invention. a. peptizer, such as ammonium oleate, soap, or an adsorptive solid, preferably finely divided, has been found helpful in effecting the dispersion during the impactive treatment. At this stage the material should be permitted to age for at least two weeks when the emulsion can be lorclaen. The oil will separate out perfectly clear and the soap or other agent will form another layer. On the other hand, the dyestufi will be mainly suspended in the water. This suspension can be used very advantageously for the dyeing of fabrics and other materials. Should it be low in dyestufi' content, it can be concentrated by D evaporation of part of the water phase. If an undesirable precipitate has been formed, it can be deflocculated or repeptized by any suitable means or it can be redispersed by the practice of the invention.

A colloidal sol of a metal is made by Bredigs arc or by any suitable method and a portion or the water is then evaporated. The concentrated material is in turn suspended in lubricating oil by the practice of the invention and the suspension is later broken when it will be found that the metallic particles will have been resuspended in the oil. This novel suspension may be advantageously used as a lubricant for machine bearings, the metallic particles having been found to have either one or the other of two important functions, dependingon the orientation of the oil. Either they adsorb to the bearing surfaces and so fill in the microscopic pits and cavities which exist in even the most highly polished surfaces or act to softly abrade to a still finer degree of smoothness.

Example 9 After the hydrolysis of magnesium hydroxide a given quantity is. subjected to impactive treatment in accordance with this invention. Heat and preliminary agitation, in this instance, are not essential. The improvement in the material as a result of this treatment may be demonstrated by the following comparative tests.

, droxide particles of each of -Into the graduate shown in Fig. 14 is poured a sample of the raw material obtained directly by hydrolysis, into the graduate shown in Fig. is poured a sample obtained by treating a given quantity of the raw material in a colloid mill of the type employing both high shearing stress and high beating action, and into the graduate shown in Fig. 16 is poured the sample treated in accordance with this invention. These three specimens are permitted to stand undisturbed in the graduates for a period of six months when they will present the appearance illustratedin said figures. The untreated product (Fig. 14) shows a sedimentation of 45%, the product obtained by the colloid mill treatment (Fig. 15) shows a sedimentation of 82%, and the product obtained by the treatment of the invention (Fig. 16) shows a sedimentation of 91.5%. Conversely stated, the untreated product has precipitated to the extent of showing 55% of its bulk as clear water, the product obtained by the colloid mill treatment has precipitated to the extent of showing 18% of its bulk as clear water, and the material obtained by the treatment of the invention has precipitated only to the extent of showing 8.5% of its bulk as clear water. It is of course understood that all three specimens should be of equal ratio of solid to liquid. Slight shaking will redisperse the magnesium hythe three specimens, but again the untreated product (Fig. 14) and the product obtained by the colloid mill treatment (Fig. 15) will precipitate out much sooner than the product obtained by the treatment or the invention (Fig. 16). In this connection it is to be particularly noted that the total sedimentations illustrated occur after a standing period of one ortwo days in the case of the UH- treated product (Fig. 14), after a standing period of two to three weeks in the case of the product obtained by the colloid mill treatment (Fig. 15), and after a standing period of about six months in the case of the product obtained by the treatment of the invention (Fig. 16).

Example 10 A given quantity of sulphur is pulverized or product superior in many respects to corresponding products now obtainable. In the usual manher, the larger particles of this new product may be separated out by elutriation and the finer material thereafter concentrated by evaporation. Proper peptizing agents may also be added to promote dispersion. v

Example 11 A sample of raw distillate of an alcoholic beverage is subjected to impactive treatment in accordance with this invention, preferably at slightly raised temperature and with applied pressure to prevent evaporation. Subsequeht agitation in the presence of an adsorptive agent such as charcoal and filtrationwill yield a beverage in which a noted increase of esterification will be found upon analysis. Taste and bouquet are likewise improved.

It is desired to have it understood that the invention is not limited to the exact procedures which have been described.

What is claimed is:

l. The'method of producing suspensions of a material in liquid comprising substantially confining against movement in all directions said liquid and material in a plurality of connected small unit volumes and subjecting each of said small unit volumes simultaneously to a pounding action to produce rapidly recurring impact disruptive shocks.

2. The method of producing suspensions in a fluid comprising substantially confining against movement in all directions a mixture of said fluid and the material to be suspended therein into a plurality of substantially enclosed and connected adjacent unit volumes and simultaneously subjecting all of said unit volumes to rapidly recurring impact disruptive shocks.

3. The method of producing suspensions in an outer phase liquid comprising, subjecting a mixture of said liquid and the material to' be suspended therein to rapidly recurring disruptive impacts delivered simultaneously to 'a plurality of small separated masses of said mixture, substantially confined against movement in all directions.

l. The method of producing emulsions comprising subjecting the materials to be emulsified while substantially separated into predetermined small unit spaces to a series of rapidly recurring impact disruptive shocks delivered simultaneously throughout said unit spaces wherein said materials are substantially confined against movement-in all directions.

5. The method of forming emulsions from the mixture of an outer phase liquid and another substance, comprising dividing the mixture into small substantially isolated unit volumes, causing the small unit volumes to bodily move, applying impacting forces against said moving volumes and in opposition to the movement thereof, and reversing the direction of said movement and said impacting forces at'a rapid rate, while confining the liquid and substance within said unit volumes against substantial flow in any direction due to. the application of said impacting forces thereto whereby said liquid and substance in said unit volumes are subjected to a pounding action.

SAMUEL JOSEPH WYNN. 

